A multilevel factorial design of 23 with 12 experiments was developed for the preparation of cellulose nanocrystals (CNC) from Agave tequilana Weber var. Azul bagasse. The studied parameters were acid type (H2SO4 and HCl), acid concentration (60 and 65 wt% for H2SO4, 2 and 8N for HCl) temperature (40 and 60°C for H2SO4, 50 and 90°C for HCl), and hydrolysis time (40, 55 and 70 min for H2SO4, 30, 115 and 200 min for HCl). The obtained CNC were physical and chemically characterized using dynamic light scattering (DLS), atomic force microscopy (AFM), Fourier-transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XDR) techniques. The size and morphology of A. tequilana CNC strongly depend on the acid type and hydrolysis parameters. The shortest CNC were obtained with H2SO4 (65 wt%, 40 °C, and 70 min) had a length of 137 ± 68 nm, width 33 ± 7 nm, and height 9.1 nm, whereas the shortest CNC obtained with HCl (2 N, 50 °C and 30 min) had a length of 216 ± 73 nm, width 69 ± 17 nm, and height 8.9 nm. CNC prepared from H2SO4 resulted shorter and thinner than those obtained with HCl. The total sulfate groups content in CNC obtained with H2SO4 increase with time agree to CSG=aebt, and increases with temperature and acid concentration.